JP2008174649A - Separation method for high-temperature high-pressure water and oil and its separation apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To efficiently separate an oil and water while recovering thermal energy by a relatively simple step. <P>SOLUTION: The high-temperature high-pressure water containing the oil comprising a heavy oil, a middle distillate, a light oil and a gas is firstly reduced to a predetermined temperature and pressure by a first separation means 11. Thereby, the heavy oil is retained in a liquid phase state with a part of the high-temperature high-pressure water, and the middle distillate, the light oil and the gas are made to be in a vapor phase state with a remained part of the high-temperature high-pressure water, and separated. Then, the heavy oil with the part of the high-temperature high-pressure water, separated by the first separation means 11, is reduced to a predetermined temperature and pressure by a second separation means 12. Thereby, the heavy oil is retained in a liquid phase state and the high-temperature high-pressure water is made to be in a vapor phase state, and separated. Further, the middle distillate, the light oil and the gas with the remained part of the high-temperature high-pressure water, separated by the first separation means 11, are reduced to a predetermined temperature and pressure by a third separation means 13. Thereby, the gas is retained in a vapor phase state and the middle distillate, the light oil and the high-temperature high-pressure water are made to be in a liquid phase state, and separated. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention uses high-temperature and high-pressure water composed of supercritical water or subcritical water, and reforms petroleum asphalt or the like into oils composed of heavy oil, medium oil, light oil, and gas, The present invention relates to a method for separating high-temperature and high-pressure water and oil, and a separation apparatus for the method.

Conventionally, after reforming heavy hydrocarbons such as vacuum residual oil and heavy crude oil in high-temperature and high-pressure water consisting of supercritical water or subcritical water, coal is separated into light product oil and water. (For example, refer patent document 1), a reforming plant (for example, refer patent document 2), etc. are disclosed. In the coal continuous conversion apparatus disclosed in Patent Document 1, carbon monoxide is supplied as a fluid gas together with water in a supercritical state to a fluid medium in a fluidized bed type reaction tower formed so as to be maintained in a supercritical state. The supercritical water is gradually reduced and cooled in a fractionation apparatus connected to the reaction tower, and iron oxide is mainly used in an oil reformer provided between the fluidized bed type reaction tower and the fractionation apparatus. The sintered particles having an average particle size of 0.3 to 5 mm as a component are filled. In addition, the fluidized medium of the fluidized bed type reaction tower is a sintered granule having an average particle size of 0.3 to 5 mm mainly composed of iron oxide, and the fractionator is composed of a heavy oil separator, a medium oil separator, A light oil separator, and the oil reformed by the oil reformer is depressurized and cooled in the order of the heavy separator, the medium separator, and the light separator.
In the coal continuous conversion apparatus constructed in this way, carbon monoxide is supplied to the pulverized coal in the fluidized state together with the water in the supercritical state from the lower part of the fluidized bed type reaction tower formed so as to be maintained in the supercritical state. If the oil produced by lightening the coal is further lightened by using the sintered particles in the oil reformer as a catalyst, it is converted into heavy oil, medium oil and light oil by the fractionator. It comes to be separated.

On the other hand, in the reforming plant described in Patent Document 2, the object to be treated is desulfurized by a hydrothermal reaction in the desulfurization reactor, and the treated product of the desulfurization reactor is lower than the treatment temperature of the desulfurization reactor in the low viscosity reactor. The viscosity is reduced by a hydrothermal reaction at a high processing temperature, and the oil content is separated as a reformed fuel from the processed product of the viscosity reduction reactor by the oil content separator. Further, the processing object to be supplied to the desulfurization reactor is preheated by exchanging heat between the processing object of the low viscosity reactor and the processing object to be supplied to the desulfurization reactor.
In the reforming plant configured as described above, the energy consumption required for the reforming process of the object to be processed is performed since the desulfurization process having a relatively low processing temperature is followed by the viscosity reducing process having a relatively high processing temperature. Can be reduced.
Japanese Patent No. 3402353 (Claims 1 to 3, paragraphs [0005] and [0006]) JP 2004-339443 A (claims 1 and 2, paragraph [0032])

However, in the fractional distillation apparatus in the coal continuous conversion apparatus shown in the above-mentioned conventional patent document 1, since a method for recovering thermal energy is not shown, the energy efficiency is lowered and the energy consumption is increased. was there.
Moreover, in the reforming plant shown in the above-mentioned conventional patent document 2, the method for separating water and produced oil is insufficient, and the recovered water forms part of the produced oil and emulsion, and the subsequent water There was a problem that processing and oil recovery were complicated.
Furthermore, in the reforming plant shown in the above-mentioned conventional patent document 2, there is a problem that heavy components contained in the product oil adhere to the pressure control valve and the heat exchanger, thereby reducing the controllability and performance. there were.
An object of the present invention is to provide a high-temperature and high-pressure water-oil separation method and a separation apparatus that can efficiently separate oil and water while recovering thermal energy by a relatively simple process. .
Another object of the present invention is to efficiently remove oil and water without degrading the controllability of a device that lowers the pressure, such as a pressure regulating valve, and without degrading the performance of a device that lowers the temperature, such as a heat exchanger. An object of the present invention is to provide a method for separating high-temperature and high-pressure water and oil, which can be separated, and a separation apparatus therefor.

  As shown in FIG. 1, the invention according to claim 1 is an oil component comprising heavy oil, medium oil, light oil and gas obtained by reforming with high-temperature and high-pressure water comprising supercritical water or subcritical water. The high-temperature high-pressure water containing water is reduced to a predetermined temperature within the range of 300 to 450 ° C. and reduced to a predetermined pressure within the range of 5 to 22 MPa in the first separation means 11, whereby heavy oil in the oil content is reduced. A step of separating the middle oil, light oil and gas, which remain in a liquid phase together with a part of the high-temperature and high-pressure water and in the gas phase together with the remainder of the high-temperature and high-pressure water, The separated heavy oil together with a part of the high-temperature high-pressure water is lowered by the second separation means 12 to a predetermined temperature within the range of 100 to 350 ° C. and to a predetermined pressure within the range of 0.1 to 4 MPa. By leaving the heavy oil in the liquid phase, A phase separation process, and the intermediate oil, light oil and gas separated by the first separation means 11 together with the remainder of the high-temperature and high-pressure water by the third separation means 13 within a predetermined range of 0 to 50 ° C. Reducing the temperature to a predetermined pressure within the range of 1 to 10 MPa, leaving the gas in a gas phase and separating the medium oil, light oil and high-temperature and high-pressure water into a liquid phase. This is a method for separating high temperature and high pressure water and oil.

In the method for separating high-temperature and high-pressure water and oil content described in claim 1, first, the oil comprises heavy oil, medium oil, light oil and gas modified by high-temperature and high-pressure water comprising supercritical water or subcritical water. By lowering the oil content to a predetermined temperature that is lower than that at the time of reforming but relatively high at the first separation means 11 and to a predetermined pressure that is lower than that at the time of reforming but relatively high, the heavy oil Is kept in a liquid phase with a part of the high-temperature high-pressure water, and the medium oil, light oil and gas are separated in a gas-phase state together with the rest of the high-temperature high-pressure water.
Next, the heavy oil separated together with a part of the high-temperature high-pressure water by the first separation means 11 is lowered to a predetermined temperature lower than that of the first separation means 11 by the second separation means 12, and the first separation means 11. By lowering the pressure to a lower predetermined pressure, the high-temperature and high-pressure water physically dissolved in the heavy oil is evaporated and separated from the heavy oil. Even if the high-temperature and high-pressure water separated from the heavy oil is passed through a device that lowers the temperature (for example, a heat exchanger), heavy oil with high viscosity does not adhere to the heat exchanger. The thermal energy possessed by the high-temperature and high-pressure water can be efficiently recovered without degrading the performance.
On the other hand, the medium oil, light oil and gas and the remainder of the high-temperature high-pressure water separated by the first separation means 11 are lowered to a predetermined temperature lower than the first separation means 11 by the third separation means 13, and the second Gas-liquid separation that separates into a gas phase (gas) and a liquid phase (water, medium oil and light oil) by lowering to a predetermined pressure lower than 1 separation means 11, water, medium oil and light oil, The oil and water are separated at the same time into gas, medium oil, light oil and water. Even if the medium oil, light oil and gas separated from the heavy oil and the remainder of the gas and the high-temperature high-pressure water are passed through a device (for example, a heat exchanger) that lowers the temperature to a predetermined temperature of the third separation means, this heat Since heavy oil with high viscosity does not adhere to the exchanger, it is possible to efficiently recover the thermal energy possessed by the remainder of the medium oil, light oil, gas, and high-temperature high-pressure water without degrading the performance of the heat exchanger. Moreover, even if the medium oil, light oil and gas separated from the heavy oil and the remainder of the gas and the high-temperature high-pressure water are passed through a device (for example, a pressure control valve) for reducing the pressure to a predetermined pressure of the third separation means 13, this pressure Since heavy oil with high viscosity does not adhere to the regulating valve, the controllability of the pressure regulating valve is not lowered. Furthermore, since the components mainly contained in heavy oil such as asphaltenes and resins that cause the formation of emulsion are separated by the first separation means 11, the oil-water separation for separating water from medium oil and light oil is performed. In addition, it is difficult to form an emulsion, and water can be efficiently separated from medium oil and light oil.

The invention according to claim 2 is the invention according to claim 1, and further supplies high-temperature and high-pressure water in a vapor phase separated by the second separation means 12 to the third separation means 13 as shown in FIG. 2. The method further includes the step of:
In the method for separating high-temperature and high-pressure water and oil described in claim 2, when the pressure in the second separation means 12 is higher than the pressure in the first separation means 11, the second separation means 12 separates from the heavy components. The high-temperature and high-pressure water that has become the steam is lowered to a predetermined pressure and then supplied to the third separation means 13. Thereby, the thermal energy of the high-temperature high-pressure water that has become steam can be further recovered by the third separation means 13.

The invention according to claim 3 is the invention according to claim 1, and, as shown in FIG. 3, two systems of the second separation means 12 and 112 are provided in parallel with each other, and these two systems of the second separation means. 12, 112 are configured to be used alternately.
The heavy oil separated together with a part of the high-temperature high-pressure water by the first separation means 11 is lowered to a predetermined temperature lower than the first separation means 11 by the second separation means 12 and from the first separation means 11. The pressure is lowered to a low predetermined pressure. That is, by reducing the pressure of the heavy oil separated together with a part of the high-temperature high-pressure water with a device (for example, a pressure regulating valve) that lowers the pressure of the second separation means 12 to a predetermined pressure, the temperature is also predetermined The temperature is lowered to Since heavy oil with high viscosity passes through each device such as the pressure regulating valve, the heavy oil may adhere to each device or the controllability of the pressure regulating valve may be reduced. For this reason, in the method for separating high-temperature and high-pressure water and oil content described in claim 3, two systems of the second separation means 12 and 112 are provided in parallel with each other, and based on the pressure difference before and after the pressure regulating valve every predetermined time. The two systems of the second separation means 12 and 112 are alternately used, and the devices such as the pressure regulating valves of the second separation means 12 and 112 that are not used are washed.

  As shown in FIG. 1, the invention according to claim 4 is an oil component comprising heavy oil, medium oil, light oil and gas obtained by reforming with high-temperature and high-pressure water comprising supercritical water or subcritical water. The high-temperature high-pressure water containing water is lowered to a predetermined temperature in the range of 300 to 450 ° C. and lowered to a predetermined pressure in the range of 5 to 22 MPa, whereby heavy oil in the oil component is combined with a part of the high-temperature high-pressure water. The first and second separation means 11 for separating the middle oil, light oil and gas, which remain in the liquid phase state, into a gas phase together with the remainder of the high-temperature and high-pressure water, and the remaining oil are separated by the first separation means 11. The heavy oil is brought into a liquid state by lowering the heavy oil together with a part of the high-temperature high-pressure water to a predetermined temperature in the range of 100 to 350 ° C. and to a predetermined pressure in the range of 0.1 to 4 MPa. 2nd part to leave high temperature and high pressure water in the gas phase The medium oil, light oil and gas separated by the means 12 and the first separation means 11 are lowered to a predetermined temperature within the range of 0 to 50 ° C. together with the remainder of the high-temperature high-pressure water and within the range of 1 to 10 MPa. By reducing the pressure to a predetermined pressure, the high-temperature and high-pressure water and the oil component are provided with the third separation means 13 that keeps the gas in a gas phase and separates the medium oil, light oil and high-temperature and high-pressure water into a liquid phase. Separation device.

In the high-temperature and high-pressure water and oil content separation apparatus according to claim 4, firstly, the high-temperature and high-pressure water comprising supercritical water or subcritical water is reformed, and consists of heavy oil, medium oil, light oil and gas. By lowering the oil content to a predetermined temperature that is lower than that at the time of reforming but relatively high at the first separation means 11 and to a predetermined pressure that is lower than that at the time of reforming but relatively high, the heavy oil Is kept in a liquid phase with a part of the high-temperature high-pressure water, and the medium oil, light oil and gas are separated in a gas-phase state together with the rest of the high-temperature high-pressure water.
Next, the temperature of the second separation means 12 is lowered to a predetermined temperature lower than that of the first separation means 11 and the pressure is lowered to a predetermined pressure lower than that of the first separation means 11, whereby high-temperature and high-pressure water physically dissolved in heavy oil is evaporated. Separated from heavy oil. Thus, even if the high-temperature and high-pressure water separated from the heavy oil is passed through a device (for example, a heat exchanger) that lowers the temperature of the second separation means 12, the heavy oil having a high viscosity does not adhere to the heat exchanger. Therefore, the thermal energy possessed by the high-temperature and high-pressure water can be efficiently recovered without degrading the performance of the heat exchanger.
On the other hand, the medium oil, light oil and gas and the remainder of the high-temperature high-pressure water separated by the first separation means 11 are lowered to a predetermined temperature lower than the first separation means 11 by the third separation means 13, and the second Gas-liquid separation that separates into a gas phase (gas) and a liquid phase (water, medium oil and light oil) by lowering to a predetermined pressure lower than 1 separation means 11, water, medium oil and light oil, The oil and water are separated at the same time into gas, medium oil, light oil and water. Even if it passes the apparatus (for example, heat exchanger) which lowers | remains medium oil, light oil and gas and high temperature / high pressure water which were isolate | separated from heavy oil to the predetermined temperature of the 3rd separation means 13 by this, Since heavy oil with high viscosity does not adhere to the heat exchanger, it is possible to efficiently recover the thermal energy of the remainder of the medium oil, light oil, gas, and high-temperature high-pressure water without degrading the performance of the heat exchanger. Further, even if the medium oil, light oil and gas separated from the heavy oil and the remainder of the high-temperature high-pressure water are passed through a device (for example, a pressure regulating valve) that lowers the predetermined pressure of the third separation means 13, this pressure Since heavy oil with high viscosity does not adhere to the regulating valve, the controllability of the pressure regulating valve is not lowered. Furthermore, since the components mainly contained in heavy oil such as asphaltenes and resins that cause the formation of emulsion are separated by the first separation means 11, the oil-water separation for separating water from medium oil and light oil is performed. In addition, it is difficult to form an emulsion, and water can be efficiently separated from medium oil and light oil.

The invention according to claim 5 is the invention according to claim 4, and further supplies high-temperature and high-pressure water in the vapor phase separated by the second separation means 12 to the third separation means 13 as shown in FIG. 2. The apparatus further includes supply means for performing the above operation.
In the high-temperature high-pressure water and oil content separation apparatus according to claim 5, when the pressure in the second separation means 12 is higher than the pressure in the first separation means 11, the second separation means 12 separates from the heavy components. The high-temperature and high-pressure water that has become the steam is lowered to a predetermined pressure and then supplied to the third separation means 13. Thereby, the thermal energy of the high-temperature high-pressure water that has become steam can be further recovered by the third separation means 13.

The invention according to claim 6 is the invention according to claim 4, and further, as shown in FIG. 3, two systems of the second separation means 12 and 112 are provided in parallel with each other, and these two systems of the second separation means. 12, 112 are configured to be used alternately.
The heavy oil separated together with a part of the high-temperature high-pressure water by the first separation means 11 is lowered to a predetermined temperature lower than the first separation means 11 by the second separation means 12 and from the first separation means 11. The pressure is lowered to a low predetermined pressure. That is, the pressure of the heavy oil separated together with a part of the high-temperature high-pressure water is lowered to a predetermined pressure by a device (for example, a pressure regulating valve) that lowers the pressure of the second separation means 12, and the temperature is also predetermined. The temperature is lowered to Since heavy oil with high viscosity passes through each device such as the pressure regulating valve, the heavy oil may adhere to each device or reduce the controllability of the pressure regulating valve. For this reason, in the method for separating high-temperature and high-pressure water and oil content described in claim 3, two systems of the second separation means 12 and 112 are provided in parallel with each other, and based on the pressure difference before and after the pressure regulating valve every predetermined time. The two systems of the second separation means 12 and 112 are alternately used, and the devices such as the pressure regulating valves of the second separation means 12 and 112 that are not used are washed.

According to the present invention, high-temperature and high-pressure water containing oil consisting of heavy oil, medium-weight oil, light oil and gas is lowered to a predetermined temperature and pressure by the first separation means, so that the heavy oil is heated to high-temperature and high-pressure. The heavy oil separated in the first separation means is separated from the high-temperature and high-pressure water by leaving it in a liquid phase with a part of the water and separating the intermediate oil, light oil and gas in the gas-phase state with the remainder of the high-temperature and high-pressure water. The heavy oil is kept in the liquid phase and the high-temperature and high-pressure water is separated in the gas phase by lowering the temperature to a predetermined temperature and pressure by the second separation means. The separated medium oil, light oil, and gas together with the remainder of the high-temperature high-pressure water are lowered to a predetermined temperature and pressure by the third separation means, so that the gas remains in a gas phase state and the medium oil, light oil And high-temperature and high-pressure water separated in a liquid phase. It is possible to efficiently recovered thermal energy can be efficiently separated and oil and water.
In addition, the oil content can be efficiently reduced without degrading the controllability of the equipment (for example, pressure regulating valve) that lowers the pressure of each separation means and without reducing the performance of the equipment (for example, heat exchanger) that lowers the temperature of each separation means. And water can be separated. In addition, since components mainly contained in heavy oil such as asphaltenes and resins that cause emulsion formation are separated by the first separation means, water, medium oil and light oil are separated by the third separation means. It is difficult to form an emulsion during oil-water separation, and water can be efficiently separated from medium oil and light oil.

In addition, when high-temperature and high-pressure water in a gas phase separated by the second separation means is supplied to the third separation means, if the pressure in the second separation means is higher than the pressure in the first separation means, the second separation means Since the high-temperature and high-pressure water that has become water vapor separated from the heavy component is supplied to the third separation means after being lowered to a predetermined pressure, the third separation means further supplies the thermal energy of the high-temperature and high-pressure water that has become water vapor. Can be recovered.
In addition, if two systems of the second separation means are provided in parallel with each other, and these two systems of second separation means are used alternately, the pressure of the second separation means is increased by heavy oil having a high viscosity passing through one of the second separation means. When the controllability of the device for adjusting the pressure (for example, the pressure regulating valve) is lowered, the use of the one second separation means is stopped and the other second separation means is used. As a result, it is possible to continuously separate the high-temperature and high-pressure water and the oil component of the present invention by washing each device such as the pressure regulating valve of one of the second separation means that has stopped using.

Next, the best mode for carrying out the present invention will be described with reference to the drawings.
<First Embodiment>
As shown in FIG. 1, the high-temperature high-pressure water / oil separation device is composed of heavy oil, medium oil, light oil and gas obtained by reforming with high-temperature high-pressure water consisting of supercritical water or subcritical water. The high-temperature high-pressure water containing the oil component is reduced to a predetermined temperature and reduced to a predetermined pressure, so that the heavy oil in the oil component remains in a liquid phase together with a part of the high-temperature high-pressure water and is the remaining oil content First separation means 11 for separating oil, light oil and gas in a gas phase together with the remainder of the high-temperature high-pressure water, and heavy oil separated by the first separation means 11 together with a part of the high-temperature high-pressure water together with a predetermined amount The first separation unit 11 and the second separation unit 12 separate the heavy oil in the liquid phase and the high temperature and high pressure water in the gas phase by lowering the temperature to a predetermined pressure. Medium oil, light oil and gas, together with the remainder of the high-temperature high-pressure water By lowering lowered and a predetermined pressure to a temperature, and a third separation means 13 for leaving the life and death wood containing oil vapor phase gas, and the light oil and high temperature and high pressure water to liquid phase separation. Examples of substances that can be reformed with a reformer using supercritical water or subcritical water include petroleum asphalt and heavy crude oil. The temperature of the supercritical water or subcritical water in the reformer is preferably higher than 400 ° C. and lower than 550 ° C., and the pressure is preferably higher than 15 MPa and lower than 30 MPa. Further, the boiling point of heavy oil exceeds 360 ° C in terms of atmospheric pressure, the boiling point of medium oil exceeds 180 ° C and below 360 ° C, and the boiling point of light oil exceeds 40 ° C and below 180 ° C. is there.

  The first separation means 11 includes a first pressure regulating valve 11b that lowers the pressure and temperature of high-temperature and high-pressure water containing oil components consisting of heavy oil, medium oil, light oil, and gas, and the pressure by the first pressure regulating valve 11b. And a first sealed container 11c in which high-temperature and high-pressure water containing an oil component consisting of heavy oil, medium oil, light oil and gas whose temperature has been lowered is stored. One end of the first pressure regulating valve 11b is provided in the middle of the supply pipe 11a connected to the reformer, and the other end of the supply pipe 11a is connected to the first sealed container 11c. The high-temperature high-pressure water containing oil composed of heavy oil, medium oil, light oil and gas reformed by the reformer is lowered to a predetermined temperature within the range of 300 to 450 ° C. by the first separation means 11. At the same time, the pressure is lowered to a predetermined temperature in the range of 5 to 22 MPa. Here, the temperature of the high-temperature high-pressure water containing oil components consisting of heavy oil, medium oil, light oil and gas is lowered to a predetermined temperature within the range of 300 to 450 ° C., and the pressure is within the range of 5 to 22 MPa. The reason why the temperature is lowered to a predetermined temperature is to obtain a high recovery rate of heat energy and a high recovery rate of light oil and medium oil. In order to obtain a higher recovery rate of heat energy and a higher recovery rate of light oil and medium oil, the temperature is lowered to a predetermined temperature within the range of 340 to 420 ° C., and the pressure is 10 to 20 MPa. Preferably, the pressure is lowered to a predetermined pressure within the range. When the pressure is lowered to 10 MPa, the temperature is lowered to a predetermined temperature within a range of 340 to 420 ° C., and when the pressure is lowered to 15 MPa, the temperature is lowered to a predetermined temperature within a range of 360 to 420 ° C. When the temperature is lowered to 20 MPa, the temperature is more preferably lowered to a predetermined temperature within the range of 380 to 420 ° C.

  The second separation means 12 has a predetermined pressure with heavy oil discharged from the first sealed container 11c provided at a lower branch pipe 12a having one end connected to the lower end of the first sealed container 11c together with a part of high-temperature high-pressure water. And the second main pressure regulating valve 12b for lowering to a predetermined temperature and the heavy oil connected to the other end of the lower branch pipe 12a and having the pressure lowered by the second main pressure regulating valve 12b together with a part of the high-temperature high-pressure water. The second airtight container 12c and the second lower airtight pipe 12d connected to the lower end of the second airtight container 12c are adjusted to adjust the pressure in the second airtight container 12c and are discharged from the second airtight container 12c. The second lower pressure adjusting valve 12e for adjusting the discharge amount of the quality oil and the second upper discharge pipe 12f connected to the upper end of the second sealed container 12c are used to adjust the pressure in the second sealed container 12c and the second. 2 And a second upper pressure regulating valve 12g for adjusting the discharging amount of high-temperature and high-pressure water vapor state discharged from closed container 12c. A lower heat exchanger 12h for recovering thermal energy from the high-temperature and high-pressure water in the gas phase is provided on the downstream side of the second upper pressure adjusting valve 12g of the second upper discharge pipe 12f.

  The heavy oil discharged from the lower end of the first sealed container 11c is a second main pressure regulating valve 12b, a second lower pressure regulating valve 12e and a second upper pressure regulating valve of the second separating means 12 together with a part of the high-temperature high-pressure water. With 12 g, the temperature is lowered to a predetermined temperature within a range of 100 to 350 ° C., and at a predetermined pressure within a range of 0.1 to 4 MPa. Here, the pressure adjustment valves 12b, 12e, and 12g reduce the temperature as well as the pressure of heavy oil or the like due to adiabatic expansion accompanying decompression. A part of the high-temperature high-pressure water discharged from the lower end of the first sealed container 11c is contained in a state of being physically dissolved in heavy oil. Here, the heavy oil was lowered to a predetermined temperature within the range of 100 to 350 ° C. together with a part of the high-temperature high-pressure water, and the heavy oil was reduced to the predetermined pressure within the range of 0.1 to 4 MPa. This is to prevent the heavy oil volume from significantly increasing due to bumping of high-temperature and high-pressure water physically dissolved in the water, thereby facilitating handling of the heavy oil. Also, since the melting point of heavy oil is as high as 100-250 ° C, when water is mixed in heavy oil, the temperature is lowered by reducing the pressure to atmospheric pressure, and the heavy oil solidifies and blocks the piping. May end up. For this reason, it is preferable to reduce the heavy oil together with a part of the high-temperature high-pressure water to a relatively high temperature of 150 ° C. or higher, although it is lower than the temperature in the first sealed container 11 c by the second separation means 12. Specifically, when the pressure is lowered to 4 MPa, the temperature is lowered to a predetermined temperature within a range of 250 to 350 ° C., and when the pressure is lowered to 1 MPa, the temperature is lowered to a predetermined temperature within a range of 180 to 350 ° C. When the pressure is reduced to 0.1 MPa, the temperature is preferably lowered to a predetermined temperature within the range of 120 to 350 ° C. In addition, if inert gas etc. are supplied to a 2nd airtight container, the order of the 2nd upper pressure regulating valve and lower heat exchanger which were provided in the 2nd upper discharge pipe can be reversed.

  The third separation means 13 is provided in the upper branch pipe 13a, one end of which is connected to the upper end of the first sealed container 11c, and the medium oil, light oil and gas discharged from the upper end of the first sealed container 11c The main heat exchanger 13b that recovers the heat energy by lowering the temperature to the first predetermined temperature together with the remaining portion of the main heat exchanger 13b is provided downstream of the main heat exchanger 13b of the upper branch pipe 13a, and the temperature is lowered by the main heat exchanger 13b. A third main pressure regulating valve 13c for lowering the medium oil, light oil and gas to a predetermined pressure together with the remainder of the high-temperature high-pressure water, and a third main pressure regulating valve 13c provided on the downstream side of the third main pressure regulating valve 13c of the upper branch pipe 13a. The sub heat exchanger 1 recovers thermal energy by lowering the medium oil, light oil and gas whose pressure has been reduced by the main pressure regulating valve 13c to the second predetermined temperature together with the remaining high-temperature high-pressure water. Has a d, wood containing oil temperature is lowered by being connected to the other end of the upper branch pipe 13a sub heat exchanger 13d, and a third closed container 13e for storing light oil and gas with the balance of high temperature and high pressure water. A third lower discharge pipe 13f is connected to the lower end of the third closed container 13e, and the third lower discharge pipe 13f adjusts the pressure in the third closed container 13e and is discharged from the third closed container 13e. A third lower pressure regulating valve 13g is provided for adjusting the discharge amount of the water in the phase state (those in which the temperature and pressure of the high-temperature high-pressure water are reduced). A third upper discharge pipe 13h is connected to the upper end of the third closed container 13e, and the pressure in the third closed container 13e is adjusted and discharged from the third closed container 13e in the middle of the third upper discharge pipe 13h. A third upper pressure adjustment valve 13i is provided for adjusting the amount of gas discharged. Further, a third middle discharge pipe 13j is provided at the center in the vertical direction of the third sealed container 13e. The pressure in the third sealed container 13e is adjusted to the third middle discharge pipe 13j from the third sealed container 13e. A third middle pressure adjusting valve 13k is provided for adjusting the discharge amount of the medium oil and light oil discharged.

  The main heat exchanger 13b, the third main pressure regulating valve 13c, the sub heat exchanger 13d, the third lower pressure regulating valve 13g, the third upper pressure regulating valve 13i, and the third middle pressure regulating valve 13k are used to form a third sealed container 13e. The temperature inside is lowered to a predetermined temperature in the range of 0 to 50 ° C., preferably 0 to 30 ° C., and the pressure in the third sealed container 13e is 1 to 10 MPa, preferably in the range of 1 to 4 ° C. The pressure is lowered to The reason why the temperature in the third sealed container 13e is lowered to a predetermined temperature in the range of 0 to 50 ° C. and the pressure in the third sealed container 13e is lowered to a predetermined pressure in the range of 1 to 10 MPa is the first This is to recover the thermal energy of the medium oil, light oil, and gas discharged from the sealed container 11c, and to ensure that the medium oil, light oil, and high-temperature high-pressure water are in a liquid phase state. Further, if the pressure in the third sealed container 13e is low, a part of the light oil moves to the gas side (gas phase side), and subsequent recovery of the light oil becomes difficult. The pressure was 1 MPa or more. Furthermore, the lower the temperature in the third sealed container 13e, the smaller the transition of light oil or water (those in which the temperature and pressure of the high-temperature high-pressure water is reduced) to the gas side (gas phase side). The lowest possible temperature in the range is desirable. If the main heat exchanger can achieve sufficient cooling, the sub heat exchanger can be omitted.

A method for separating high-temperature and high-pressure water and oil using the thus configured separation device will be described.
First, an oil component consisting of heavy oil, medium oil, light oil and gas obtained by reforming a raw material such as petroleum asphalt with high-temperature and high-pressure water composed of supercritical water or subcritical water is a first pressure regulating valve 11b. And then stored in the first sealed container 11c. The temperature in the 1st airtight container 11c falls by pressure reduction operation by the 1st pressure regulation valve 11b. Specifically, although the temperature in the first sealed container 11c is lower than that during the reforming, it is lowered to a predetermined temperature within a relatively high range of 300 to 450 ° C. and lower than that during the reforming. The pressure is lowered to a predetermined pressure within a relatively high range of 5 to 22 MPa. As a result, the solubility of a part of the heavy oil dissolved in the high-temperature and high-pressure water is lowered, so that the heavy oil having a large specific gravity moves to the lower part of the first sealed container 11c together with a part of the high-temperature and high-pressure water. The refined oil, light oil and gas become a gas phase together with the remainder of the high-temperature and high-pressure water and move to the upper part of the first sealed container 11c. The higher the pressure in the first sealed container 11c, the higher the heat energy recovery rate. In addition, if the temperature in the first sealed container 11c is low, a part of the medium oil is also in a liquid phase and recovered together with the heavy oil. Therefore, the temperature and pressure in the first sealed container 11c are set to the above temperature. It is necessary to select appropriately in the range and pressure range.

  The heavy oil stored in the lower portion of the first sealed container 11c passes through the lower branch pipe 12a together with a part of the high-temperature and high-pressure water, and after being depressurized by the second main pressure regulating valve 12b, is stored in the second sealed container 12c. The The temperature in the 2nd airtight container 12c falls by pressure reduction operation by the 2nd main pressure regulating valve 12b. Specifically, the temperature in the second sealed container 12c is lowered to a predetermined temperature in the range of 100 to 350 ° C. lower than that in the first sealed container 11c, and is 0.1 lower than that in the first sealed container 11c. The pressure is lowered to a predetermined pressure within a range of ˜4 MPa. As a result, the high-temperature and high-pressure water physically dissolved in the heavy oil evaporates and is separated from the heavy oil, so that the heavy oil moves to the lower part of the second sealed container 12c in the liquid phase and evaporates to the gas phase. The high-temperature and high-pressure water in the state moves to the upper part of the second sealed container 12c. The heavy oil stored in the lower portion of the second sealed container 12c passes through the second lower discharge pipe 12d and is discharged after being depressurized by the second lower pressure regulating valve 12e. The high-temperature and high-pressure water in the vapor state stored in the upper part of the second sealed container 12c passes through the second upper discharge pipe 12f and is depressurized by the second upper pressure regulating valve 12g. Collected and discharged. Since the high-temperature and high-pressure water in the gas phase does not contain heavy oil, heavy oil with high viscosity does not adhere to the second upper pressure regulating valve 12g or the lower heat exchanger 12h. As a result, the thermal energy of the high-temperature and high-pressure water in the gas phase can be efficiently recovered without degrading the controllability of the second upper pressure regulating valve 12g and without degrading the performance of the lower heat exchanger 12h.

  On the other hand, the gas phase intermediate oil, light oil and gas stored in the upper part of the first sealed container 11c pass through the upper branch pipe 13a together with the remainder of the gas phase high temperature and high pressure water and are cooled by the main heat exchanger 13b. Then, the main heat energy is recovered, depressurized by the third main pressure regulating valve 13c, further cooled by the sub heat exchanger 13d and recovered, and then stored in the third sealed container 13e. The temperature in the third sealed container 13e is lowered by the main heat exchanger 13b and the sub heat exchanger 13d. Specifically, the temperature in the third sealed container 13e is lowered to a predetermined temperature in the range of 0 to 50 ° C. lower than that in the first sealed container 11c, and is 0.1 lower than in the first sealed container 11c. The pressure is lowered to a predetermined pressure within a range of 10 MPa. As a result, gas-liquid separation that separates into a gas phase (gas) and a liquid phase (water, medium oil, and light oil) and oil-water separation that separates into water, medium oil, and light oil are performed simultaneously. , Separated into gas and medium oil and light oil and water. Specifically, the main heat exchanger 13b, the third main pressure regulating valve 13c, and the sub heat exchanger 13d cool and decompress the high-temperature and high-pressure water in the vapor phase to form water, Although the light oil is cooled and depressurized to become a medium oil and a light oil in a liquid phase, the gas is stored in the third sealed container 13e in a gas phase. Then, the water having the highest specific gravity moves to the lower part of the third sealed container 13e, the gas having the lowest specific gravity moves to the upper part of the third sealed container 13e, and the liquid phase state has a specific gravity smaller than that of water and larger than that of the gas. Oil and light oil move to the center of the 3rd airtight container 13e in the up-and-down direction.

  The water stored in the lower part of the third sealed container 13e passes through the third lower discharge pipe 13f, and is discharged after being depressurized by the third lower pressure regulating valve 13g. The gas stored in the upper portion of the third sealed container 13e passes through the third upper discharge pipe 13h and is discharged after being depressurized by the third upper pressure adjusting valve 13i. Furthermore, the liquid medium state light oil and light oil stored in the vertical center of the third hermetic container 13e pass through the third middle discharge pipe 13j and are discharged after being depressurized by the third middle pressure regulating valve 13k. Thus, the main oil exchanger 13b, the third main pressure regulating valve 13c, and the sub heat exchanger together with the remainder of the high temperature and high pressure water, the medium oil, the light oil and the gas separated from the heavy oil by the first separation means 11. Even if it passes 13d, since heavy oil with high viscosity does not adhere to these heat exchangers and pressure control valves, medium oil, light oil and gas, and high-temperature and high-pressure water without deteriorating the performance of the heat exchanger The remaining heat energy can be efficiently recovered and the controllability of the pressure regulating valve is not lowered. That is, since deterioration and operation failure due to adhesion and accumulation of heavy oil on the heat exchanger and the pressure regulating valve do not occur, these performances and controllability can be maintained. Furthermore, since the components mainly contained in heavy oil such as asphaltenes and resins that cause the formation of emulsion are separated by the first separation means 11, the oil-water separation for separating water from medium oil and light oil is performed. In addition, it is difficult to form an emulsion, and water can be efficiently separated from medium oil and light oil.

<Second Embodiment>
FIG. 2 shows a second embodiment of the present invention. 2, the same reference numerals as those in FIG. 1 denote the same components.
In this embodiment, the high-temperature high-pressure water in the vapor phase separated by the second separation means 12 is supplied to the third separation means 13 by the supply means 31. The supply means 31 lowers the pressure of the high-temperature high-pressure water in the gas phase state in the second sealed container 12c provided in the communication pipe 31a and the communication pipe 31a connecting the second upper discharge pipe 12f and the upper branch pipe 13a. And a communication pressure regulating valve 31b. One end of the communication pipe 31a is connected between the second sealed container 12c and the second upper pressure regulating valve 12g in the second upper discharge pipe 12f, and the other end of the communication pipe 31a is the third main in the upper branch pipe 13a. It is connected between the pressure regulating valve 13c and the sub heat exchanger 13d. The configuration other than the above is the same as that of the first embodiment.
In the high-temperature and high-pressure water / oil separation device configured as described above, when the pressure in the second sealed container 12c is higher than the pressure in the third sealed container 13e, the high-temperature and high-pressure water in the gas phase is connected to the pressure regulating valve for communication. Since it is supplied to the sub heat exchanger 13d after being lowered to a predetermined pressure by 31b, the thermal energy possessed by the high-temperature high-pressure water can be recovered more efficiently. Since the operation other than the above is substantially the same as the operation of the first embodiment, repeated description is omitted.

<Third Embodiment>
FIG. 3 shows a third embodiment of the present invention. 3, the same reference numerals as those in FIG. 1 denote the same components.
In this embodiment, two systems of the second separation means 12 and 112 are provided in parallel with each other, that is, one second separation means 12 and the other second separation means 112 are configured identically. Specifically, one of the second separating means 12 includes a lower branch pipe 12a, a second main pressure adjustment valve 12b, a second sealed container 12c, a second lower discharge pipe 12d, and a second lower pressure adjustment valve. 12e, a second upper discharge pipe 12f, a second upper pressure adjustment valve 12g, and a lower heat exchanger 12h. The other second separation means 112 includes a lower branch pipe 112a, a second main pressure adjustment A valve 112b, a second sealed container 112c, a second lower discharge pipe 112d, a second lower pressure adjustment valve 112e, a second upper discharge pipe 112f, a second upper pressure adjustment valve 112g, and a lower heat exchanger 112h And have. One end of the lower branch pipe 112a of the other second separating means 112 is connected between the first sealed container 11c and the second main pressure regulating valve 12b in the lower branch pipe 12a of the second second separating means 12. . The configuration other than the above is the same as that of the first embodiment.

A method for separating high-temperature and high-pressure water and oil using the thus configured separation device will be described.
First, the second main pressure regulating valve 12b of one second separating means 12 is opened, the second main pressure regulating valve 112b of the other second separating means 112 is closed, and the first sealing is performed by one second separating means 12. The heavy oil discharged from the container 11c is treated together with a part of the high-temperature high-pressure water. When a predetermined time has elapsed, the second main pressure regulating valve 12b of one second separating means 12 is closed, the second main pressure regulating valve 112b of the other second separating means 112 is opened, and the other second pressure regulating valve 112b is opened. The heavy oil discharged | emitted from the 1st airtight container 11c by the 2 separation means 112 is processed with a part of high temperature high pressure water. During this time, the heavy oil with high viscosity attached to the second main pressure regulating valve 12b, the second sealed container 12c, the second lower pressure regulating valve 12e, etc. of the second separating means 12 whose use has been stopped is removed. When a predetermined time has elapsed, the second main pressure regulating valve 12b of one of the second separating means 12 is opened, and the second main pressure regulating valve 112b of the other second separating means 112 is closed, The heavy oil discharged | emitted from the 1st airtight container 11c by the 2 separation means 12 is processed with a part of high temperature high pressure water. During this time, the heavy oil with high viscosity attached to the second main pressure regulating valve 112b, the second sealed container 112c, the second lower pressure regulating valve 112e, etc. of the other second separating means 112 that has been stopped is removed. In this way, by alternately operating one second separation means 12 and the other second separation means 112 and washing each device of the second separation means on the unused side, the second main pressure regulating valve or Separation of heavy oil and high-temperature high-pressure water can be performed continuously without degrading the controllability of the second lower pressure regulating valve or the like.
In the third embodiment, the switching operation between one second separation means and the other second separation means is performed every predetermined time. However, either the second main pressure adjustment valve or the second lower pressure adjustment valve is used. A pressure sensor may be provided before or after one or both, and the switching operation of one second separation means and the other second separation means may be performed based on the detection output of the pressure sensor.

Next, embodiments of the present invention will be described in detail.
<Example 1>
Petroleum asphalt was used as a raw material, the reforming conditions with high-temperature and high-pressure water made of supercritical water, that is, the reforming temperature was 480 ° C., and the reforming pressure was 25 MPa. When the total amount of oil and high-temperature high-pressure water was 100% by weight, each component after the above reforming was set as follows. Heavy oil was 8% by weight, medium oil was 3% by weight, light oil was 2% by weight, gas was 19% by weight, and high-temperature high-pressure water was 68% by weight. The high-temperature and high-pressure water containing this oil is separated by the first separation means from the high-temperature and high-pressure water and the light oil and medium oil in the gas phase, and the heavy oil corresponding to the vacuum residue is separated in the liquid phase. The change in the separation behavior was calculated using a computer while changing the temperature condition and pressure condition of the first closed container of one separation means. The result is shown in FIG.
As is clear from FIG. 4, the higher the temperature in the first sealed container, the higher the gas phase transfer rate of water, light oil, and medium oil, but the heavy oil may also shift to the gas phase. I understand. Moreover, as the influence of the pressure, the lower the pressure in the first sealed container, the less entrainment of heavy oil on the gas phase side becomes, but the light oil of medium oil, which is one of the products, remains in the liquid phase. It turned out that it tends to become easy. Appropriate separation conditions in the first closed container inferred from these, the temperature is 380-420 ° C. when the pressure is 20 MPa, the temperature is 360-420 ° C. when the pressure is 15 MPa, It is considered that the temperature is 340 to 420 ° C. when the pressure is 10 MPa.

<Example 2>
Liquid phase heavy oil discharged from the first airtight container of the first separation means is separated together with a part of the high temperature and high pressure water by the second separation means, and the high temperature and high pressure water is separated in the gas phase state, and the heavy oil is liquefied. Separation was performed in the phase state, and the change in the separation behavior was calculated using a computer while changing the temperature condition and pressure condition of the second closed vessel of the second separation means. The result is shown in FIG.
As is clear from FIG. 5, it was found that heavy oil is in a liquid phase, and high-temperature high-pressure water increases in the rate of transition to the gas phase as the pressure decreases. In addition, when the pressure in the second sealed container is less than 0.1 MPa, the viscosity of the heavy oil is increased, and it may be difficult to handle. Therefore, the appropriate separation pressure in the second sealed container is It is estimated that it is in the range of 0.1 to 4 MPa. As for the separation temperature in the second closed vessel, the temperature is 180 to 350 ° C. when the pressure is 1 MPa, and the temperature is 250 to 350 ° C. when the pressure is 4 MPa. In order to maintain a low viscosity, it is considered that a separation operation at a higher temperature is appropriate.

<Example 3>
Gas-phase medium oil, light oil and gas discharged from the first sealed container of the first separation means are separated from the gas in the gas-phase state by the third separation means together with the remainder of the high-temperature and high-pressure water. In addition, light oil and water were separated in a liquid phase, and the change in the separation behavior was calculated using a computer while changing the temperature condition and pressure condition of the third sealed container of the third separation means. The result is shown in FIG.
As apparent from FIG. 6, it is considered that the low temperature condition side in which the pressure in the third sealed container is in the range of 1 to 4 MPa is appropriate as the separation condition in which the light oil and water hardly move to the gas phase side.

It is a block diagram which shows the high temperature / high pressure water and oil content separation apparatus of 1st Embodiment of this invention. It is a block diagram which shows the high temperature / high pressure water and oil content separation apparatus of 2nd Embodiment of this invention. It is a block diagram which shows the high temperature / high pressure water and oil-separation apparatus of 3rd Embodiment of this invention. It is a figure which shows the gaseous-phase transfer rate by the temperature change and pressure change of each oil component in a 1st separator. It is a figure which shows the gaseous-phase transfer rate by the temperature change and pressure change of each oil component in a 2nd separator. It is a figure which shows the gaseous-phase transfer rate by the temperature change and pressure change of each oil component in a 3rd separator.

Explanation of symbols

11 First Separation Unit 12, 112 Second Separation Unit 13 Third Separation Unit 31 Supply Unit

Claims (6)

The high-temperature high-pressure water containing an oil component consisting of heavy oil, medium oil, light oil and gas obtained by reforming with high-temperature high-pressure water consisting of supercritical water or subcritical water is converted into 300 by the first separation means. The heavy oil is kept in a liquid phase together with a part of the high-temperature high-pressure water by lowering to a predetermined temperature within a range of ˜450 ° C. and lowering to a predetermined pressure within a range of 5 to 22 MPa. And separating the intermediate oil, the light oil and the gas that are the remainder of the oil into a gas phase together with the remainder of the high-temperature high-pressure water, and
The heavy oil separated by the first separation means is lowered to a predetermined temperature within the range of 100 to 350 ° C. by the second separation means together with a part of the high-temperature high-pressure water, and the range of 0.1 to 4 MPa. Reducing the internal oil to a predetermined pressure, leaving the heavy oil in a liquid phase and separating the high-temperature and high-pressure water in a gas phase; and
The intermediate oil, the light oil and the gas separated by the first separation means are lowered to a predetermined temperature within a range of 0 to 50 ° C. by the third separation means together with the rest of the high-temperature high-pressure water and 1 Lowering the pressure to a predetermined pressure within a range of 10 MPa to leave the gas in a gas phase and separating the medium oil, the light oil, and the high-temperature and high-pressure water in a liquid phase, Separation method of high pressure water and oil.   The method for separating high-temperature and high-pressure water and oil components according to claim 1, further comprising a step of supplying high-temperature and high-pressure water in a gas phase separated by the second separation means to the third separation means.   The method for separating high-temperature and high-pressure water and oil components according to claim 1, wherein two systems of second separation means are provided in parallel with each other, and the two systems of second separation means are used alternately. The high temperature and high pressure water containing an oil component consisting of heavy oil, medium oil, light oil and gas obtained by reforming with high temperature and high pressure water consisting of supercritical water or subcritical water is within a range of 300 to 450 ° C. To a predetermined pressure within a range of 5 to 22 MPa, the heavy oil of the oil component is left in a liquid phase together with a part of the high-temperature high-pressure water, and the remainder of the oil component A first separation means for separating the medium oil, the light oil and the gas into a gas phase together with the remainder of the high-temperature high-pressure water;
The heavy oil separated by the first separation means is lowered together with a part of the high-temperature high-pressure water to a predetermined temperature in the range of 100 to 350 ° C. and to a predetermined pressure in the range of 0.1 to 4 MPa. A second separation means for keeping the heavy oil in a liquid state and separating the high-temperature high-pressure water in a gas-phase state by lowering,
The intermediate oil, the light oil and the gas separated by the first separation means are lowered to a predetermined temperature within a range of 0 to 50 ° C. together with the rest of the high-temperature high-pressure water and within a range of 1 to 10 MPa. High-temperature high-pressure water comprising a third separation means for keeping the gas in a gas phase state and lowering the medium oil, the light oil, and the high-temperature high-pressure water in a liquid phase state by lowering to a predetermined pressure And oil separator.   The apparatus for separating high-temperature and high-pressure water and oil according to claim 4, further comprising a supply means for supplying the high-temperature and high-pressure water in a gas phase separated by the second separation means to the third separation means.   The high-temperature high-pressure water and oil content separation device according to claim 4, wherein two systems of the second separation means are provided in parallel to each other, and the two systems of the second separation means are alternately used.

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